US2971221A - Process for curing continuous extrusions of compounded elastomers - Google Patents

Process for curing continuous extrusions of compounded elastomers Download PDF

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US2971221A
US2971221A US790234A US79023459A US2971221A US 2971221 A US2971221 A US 2971221A US 790234 A US790234 A US 790234A US 79023459 A US79023459 A US 79023459A US 2971221 A US2971221 A US 2971221A
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curing
bath
compounded
elastomeric material
elastomers
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US790234A
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Melvin A Schoenbeck
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EIDP Inc
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EI Du Pont de Nemours and Co
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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J3/00—Processes of treating or compounding macromolecular substances
    • C08J3/24—Crosslinking, e.g. vulcanising, of macromolecules
    • C08J3/247—Heating methods
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C35/00—Heating, cooling or curing, e.g. crosslinking or vulcanising; Apparatus therefor
    • B29C35/02—Heating or curing, e.g. crosslinking or vulcanizing during moulding, e.g. in a mould
    • B29C35/04—Heating or curing, e.g. crosslinking or vulcanizing during moulding, e.g. in a mould using liquids, gas or steam
    • B29C35/06—Heating or curing, e.g. crosslinking or vulcanizing during moulding, e.g. in a mould using liquids, gas or steam for articles of indefinite length
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
    • B29C48/03—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor characterised by the shape of the extruded material at extrusion
    • B29C48/05—Filamentary, e.g. strands
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
    • B29C48/03—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor characterised by the shape of the extruded material at extrusion
    • B29C48/06—Rod-shaped
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
    • B29C48/25—Component parts, details or accessories; Auxiliary operations
    • B29C48/88—Thermal treatment of the stream of extruded material, e.g. cooling
    • B29C48/91—Heating, e.g. for cross linking
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C35/00—Heating, cooling or curing, e.g. crosslinking or vulcanising; Apparatus therefor
    • B29C35/02—Heating or curing, e.g. crosslinking or vulcanizing during moulding, e.g. in a mould
    • B29C35/04—Heating or curing, e.g. crosslinking or vulcanizing during moulding, e.g. in a mould using liquids, gas or steam
    • B29C35/041—Heating or curing, e.g. crosslinking or vulcanizing during moulding, e.g. in a mould using liquids, gas or steam using liquids
    • B29C2035/042—Heating or curing, e.g. crosslinking or vulcanizing during moulding, e.g. in a mould using liquids, gas or steam using liquids other than water
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
    • B29C48/03—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor characterised by the shape of the extruded material at extrusion
    • B29C48/09—Articles with cross-sections having partially or fully enclosed cavities, e.g. pipes or channels
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29K—INDEXING SCHEME ASSOCIATED WITH SUBCLASSES B29B, B29C OR B29D, RELATING TO MOULDING MATERIALS OR TO MATERIALS FOR MOULDS, REINFORCEMENTS, FILLERS OR PREFORMED PARTS, e.g. INSERTS
    • B29K2021/00—Use of unspecified rubbers as moulding material
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29L—INDEXING SCHEME ASSOCIATED WITH SUBCLASS B29C, RELATING TO PARTICULAR ARTICLES
    • B29L2031/00—Other particular articles
    • B29L2031/26—Sealing devices, e.g. packaging for pistons or pipe joints
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2321/00—Characterised by the use of unspecified rubbers

Definitions

  • This invention is directed to a novel process for the curing of elastomers. More particularly this invention is directed to a novel process for curing a continuous length of compounded elastomer, such as an extruded gasket.
  • Continuous lengths of compounded elastomers, in such forms as tubing, coverings for wire, covering bases, and window channels are commonly formed by extrusion through a die and are cured by passage through heated chambers or, more recently, through heated liquid baths, as described in Rubber Age, 83, 88', April 1958. Since the density of the extruded article is usually quite different from that of the curing bath, rather elaborate means must be provided either for keeping the article, as it passes through the bath, from scraping the bottom (of the bath) if it is more dense than the bath liquid or from floating on the top if it is less dense. Since these means for guiding the extrudate must be operated inside the heated bath, they make the equipment rather complicated and troublesome to maintain.
  • the present invention is directed to a process for curing a continuous length of extruded elastomeric material by continuously passing it horizontally within the interface between two heated immiscible liquids, one of said liquids being substantially more dense and the other substantially less dense than the compounded elastomer being cured.
  • This assembly consists of the extruder 1 from which the compounded elastomer is delivered as a continuous extrudate 2 into the curing tank 3, a long, horizontal trough with closed ends.
  • This tank contains the two immiscible liquids as layers A and B with their interface approximately half-way between the bottom and top.
  • the tank is heated electrically with strip heaters (not shown) applied to the outside of the tank throughout its length.
  • the extrudate 2 floats at this interface without mechanical support and without the need of keeping it submerged.
  • At the far end of the tank it is raised from the bath and removed by the traction roller 4.
  • Auxiliary equipment for the tank such as drain lines, thermometers and thermoregulators, and a hood and exhaust system, are not shown.
  • Example Polychloroprene is compounded as follows and then extruded from a A-inch die at the rate of 10 ft. per min. directly into the curing bath described above, 5 ft. long; all parts are by weight.
  • This stock had a density of 1.33.
  • the lower liquid in the bath is an alloy of 58% bismuth and 42% tin, melting at 281 F. with a density of 8.7 at 68 F.
  • the upper liquid is a high-boiling polyalkylene glycol with a density of 1.04 at 68 F., with flash point of 500 F., stabilized with phenyl alpha-naphthylamine.
  • the bath is kept at 475 F. Since the extrudate moves 10 ft. per min. and the bath is 5 ft long, the extrudate is in the bath for 30 sec., which gives a good cure. After removal from the bath, the cured extrudate is washed with water to remove any adhering polyalkylene glycol. The finished product is then cut into uniform lengths or wound up on reels for storage and shipping. It has a smooth, glossy surface, free from marring.
  • This curing process may be applied to any properly compounded elastomer. Any speed at which the material is extruded from conventional equipment, up to about ft. per min. is satisfactory for passing the extrudate through the curing bath. Lower speeds are usually more practical, however, since they may be used on shorter baths to get the same residence time.
  • the bath temperature is usually between 300 and 600 F. and preferably between 450 and 500 F., although the high temperatures are entirely satisfactory, since there are no moving parts within the bath.
  • Suitable materials for denser phase are low melting alloys, usually containing tin or bismuth or both, such as Woods metal, bismuth solder and the alloy used in the example, and low melting salts, including hydrates, and very concentrated solutions of salts in water.
  • suitable materials for the upper layer vary somewhat with the elastomer but polyalkylene glycols and silicone oils are generally applicable.
  • paraflinic petroleum oils and (when suiliciently stable) fatty acid glycerides may be used and have the advantage of low cost. They may be conveniently removed from the extrudate by means of a detergent solution.
  • the bath may be heated externally by electric heaters or by gas flames or the like or internally by electric immersion heaters. If the sources of heat are Well distributed along the length of the trough, stirring is usually unnecessary, especially when an alloy is used.

Description

Feb. 14, 1961 M. A. SCHOENBECK PROCESS FOR CURING CONTINUOUS EXTRUSIONS 0F COMPOUNDED ELASTOMERS Filed Jan. 30, 1959 INVENTOR MELVIN A. SCHOENBECK PROCESS FOR CURING CONTINUOUS EXTRU- SIGNS OF COMPOUNDED ELASTOMERS Melvin A. Schoenbeck, Wilmington, Del assignor to E. I. du Pont de Nemours and Company, Wilmington, Del., a corporation of Delaware Filed Jan. 30, 1959, Ser. No. 790,234
3 Claims. (CI. 18-53) This invention is directed to a novel process for the curing of elastomers. More particularly this invention is directed to a novel process for curing a continuous length of compounded elastomer, such as an extruded gasket.
Continuous lengths of compounded elastomers, in such forms as tubing, coverings for wire, covering bases, and window channels are commonly formed by extrusion through a die and are cured by passage through heated chambers or, more recently, through heated liquid baths, as described in Rubber Age, 83, 88', April 1958. Since the density of the extruded article is usually quite different from that of the curing bath, rather elaborate means must be provided either for keeping the article, as it passes through the bath, from scraping the bottom (of the bath) if it is more dense than the bath liquid or from floating on the top if it is less dense. Since these means for guiding the extrudate must be operated inside the heated bath, they make the equipment rather complicated and troublesome to maintain.
It is, therefore, an object of the present invention to provide a novel process, requiring simple and practical equipment, for the continuous curing of continuously extruded compounded elastomer articles. These and other objects will become apparent in the following description and claims.
More specifically, the present invention is directed to a process for curing a continuous length of extruded elastomeric material by continuously passing it horizontally within the interface between two heated immiscible liquids, one of said liquids being substantially more dense and the other substantially less dense than the compounded elastomer being cured.
The equipment which may be used is shown in Figures I and II. This assembly consists of the extruder 1 from which the compounded elastomer is delivered as a continuous extrudate 2 into the curing tank 3, a long, horizontal trough with closed ends. This tank contains the two immiscible liquids as layers A and B with their interface approximately half-way between the bottom and top. The tank is heated electrically with strip heaters (not shown) applied to the outside of the tank throughout its length. The extrudate 2 floats at this interface without mechanical support and without the need of keeping it submerged. At the far end of the tank it is raised from the bath and removed by the traction roller 4. Auxiliary equipment for the tank, such as drain lines, thermometers and thermoregulators, and a hood and exhaust system, are not shown.
A representative example illustrating the present invention follows.
Example Polychloroprene is compounded as follows and then extruded from a A-inch die at the rate of 10 ft. per min. directly into the curing bath described above, 5 ft. long; all parts are by weight.
"atent -Polychloroprene p r 100.0 *Stearic acid N 0.5 Magnesium oxide 2.0 Phenyl alpha naphthylamine q Semi-reinforcing carbon black 50.0 -Di(2-ethylhexyl)sebacate- 20;.0 Zinc oxide "5.0 Z-mercaptoirnidazoline 1.0
This stock had a density of 1.33. The lower liquid in the bath is an alloy of 58% bismuth and 42% tin, melting at 281 F. with a density of 8.7 at 68 F. The upper liquid is a high-boiling polyalkylene glycol with a density of 1.04 at 68 F., with flash point of 500 F., stabilized with phenyl alpha-naphthylamine. The bath is kept at 475 F. Since the extrudate moves 10 ft. per min. and the bath is 5 ft long, the extrudate is in the bath for 30 sec., which gives a good cure. After removal from the bath, the cured extrudate is washed with water to remove any adhering polyalkylene glycol. The finished product is then cut into uniform lengths or wound up on reels for storage and shipping. It has a smooth, glossy surface, free from marring.
This curing process may be applied to any properly compounded elastomer. Any speed at which the material is extruded from conventional equipment, up to about ft. per min. is satisfactory for passing the extrudate through the curing bath. Lower speeds are usually more practical, however, since they may be used on shorter baths to get the same residence time. The bath temperature is usually between 300 and 600 F. and preferably between 450 and 500 F., although the high temperatures are entirely satisfactory, since there are no moving parts within the bath.
There is considerable latitude in the choice of both liquid components of the bath but for practical reasons they should have melting points at least 100 F. below the operating temperature and boiling points and flash points at least 25 F. above it. They should be nontoxic and without strong odor and should have no swelling action on the extrudate under operating conditions and should be stable for long periods at operating temperatures exposed to air. Suitable materials for denser phase are low melting alloys, usually containing tin or bismuth or both, such as Woods metal, bismuth solder and the alloy used in the example, and low melting salts, including hydrates, and very concentrated solutions of salts in water. The chemical classes from which suitable materials for the upper layer are selected vary somewhat with the elastomer but polyalkylene glycols and silicone oils are generally applicable. For polychloroprene and other inherently oil-resistant elastomers, paraflinic petroleum oils and (when suiliciently stable) fatty acid glycerides may be used and have the advantage of low cost. They may be conveniently removed from the extrudate by means of a detergent solution.
The bath may be heated externally by electric heaters or by gas flames or the like or internally by electric immersion heaters. If the sources of heat are Well distributed along the length of the trough, stirring is usually unnecessary, especially when an alloy is used.
As many apparently widely ditferent embodiments of this invention may be made without departing from the spirit and scope thereof, it is to be understood that this invention is not limited to the specific embodiments thereof except as defined in the appended claims.
The embodiments of the invention in which an exclusive property or privilege is claimed. are defined as follows:
I. A process for curing a continuous length of extruded compounded elastomeric material at atmospheric pressure by continuously passing said material horizontalliquids, the lower liquid layer being substantially more dense than said elastomeric material, the upper liquid layerbeing substantially less dense than said elastomeric material, but of said immiscible liquid layers having a melting point of at least 1001f. below the operating temperature and a boiling point and flash point at least 25 F. above the operating temperature, said process-being operated at a temperature within the range of 300 to 600 F. a a
2. The process of claim 1 wherein the upper liquid layer is a polyethylene glycol.
3. The process of claim I conducted at a temperature within the range of 450 to 500 F.
References Cited in-thefile of this patent v UNITED STATES PATENTS 2,553,938 Pierce May 22, 1951 UNITED STATES PATENT OFFICE CERTIFICATION OF CORRECTION Patent N20, 2,971,221 February 14, 1961 Melvin A, Schoenbeck at error appears in the above numbered patis hereby certified th hat the said Letters Patent should read as ent Zing correction and t corre- .f'clow I Column 3, line 5, for "but" read both Signed and sealed this 27th day of June 1961,,
(SEAL) Attest:
DAVID L. LADD ERNEST W. SWIDER Commissioner of Patents Attesting Officer

Claims (1)

1. A PROCESS FOR CURING A CONTINUOUS LENGTH OF EXTRUDED COMPOUNDED ELASTOMERIC MATERIAL AT ATMOSPHERIC PRESSURE BY CONTINUOUSLY PASSING SAID MATERIAL HORIZONTALLY WITHIN THE INTERFACE BETWEEN TWO HEATED IMMISCIBLE LIQUIDS, THE LOWER LIQUID LAYER BEING SUBSTANTIALLY MORE DENSE THAN SAID ELASTOMERIC MATERIAL, THE UPPER LIQUID LAYER BEING SUBSTANTIALLY LESS DENSE THAN SAID ELASTOMERIC MATERIAL, BUT OF SAID IMMISCIBLE LIQUID LAYERS HAVING A MELTING POINT OF AT LEAST 100*F. BELOW THE OPERATING TEMPERATURE AND A BOILING POINT AND FLASH POINT AT LEAST 25* F. ABOVE THE OPERATING TEMPERATURE, SAID PROCESS BEING OPERATED AT A TEMPERATURE WITHIN THE RANGE OF 300* TO 600*F.
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Cited By (14)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3051992A (en) * 1960-05-20 1962-09-04 Cabot Corp Continuous curing of polymeric materials
US3072968A (en) * 1959-11-11 1963-01-15 Rubber And Plastics Res Ass Of Heat treatment of rubber
US3373143A (en) * 1962-05-30 1968-03-12 Ici Ltd Manufacture of polyurethane solutions
US3501804A (en) * 1967-06-13 1970-03-24 Ball Brothers Co Inc Rubber curing apparatus and method
US3859247A (en) * 1970-11-20 1975-01-07 Gen Electric Pressureless cure system for chemically cross-linking ethylene containing polymers
US3946099A (en) * 1972-11-10 1976-03-23 General Electric Company Pressureless cure system for chemically cross-linking ethylene containing polymers, to form an insulated conductor
US4143106A (en) * 1977-08-15 1979-03-06 The Dow Chemical Company Continuous flood foaming of thermoplastic resin
US4155965A (en) * 1977-01-07 1979-05-22 The Dow Chemical Company Continuous submerged foaming of thermoplastic resin
US4209484A (en) * 1977-02-28 1980-06-24 Pont-A-Mousson S.A. Method of manufacturing products of cross-linked thermoplastic material
US4226816A (en) * 1977-07-16 1980-10-07 Aisin Chemical Company, Limited Method of manufacturing a clutch facing of the type used for automotive automatic transmissions
US4415518A (en) * 1981-12-21 1983-11-15 Pochurek Gerald M Continuous curing of cable
US4892544A (en) * 1988-03-07 1990-01-09 Dow Corning Wright Corporation Methods for forming hollow, porous-surfaced elastomeric bodies
US5595695A (en) * 1995-05-30 1997-01-21 Sealex Inc. Process for preparing matte finish elastomer
EP0985509A1 (en) * 1998-05-04 2000-03-15 COLMEC S.p.A. Method and apparatus for the curing of extruded sections on a bath of melted salts

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2553938A (en) * 1948-02-17 1951-05-22 American Steel & Wire Co Method and apparatus for continuously vulcanizing the rubber covering of conductors

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2553938A (en) * 1948-02-17 1951-05-22 American Steel & Wire Co Method and apparatus for continuously vulcanizing the rubber covering of conductors

Cited By (14)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3072968A (en) * 1959-11-11 1963-01-15 Rubber And Plastics Res Ass Of Heat treatment of rubber
US3051992A (en) * 1960-05-20 1962-09-04 Cabot Corp Continuous curing of polymeric materials
US3373143A (en) * 1962-05-30 1968-03-12 Ici Ltd Manufacture of polyurethane solutions
US3501804A (en) * 1967-06-13 1970-03-24 Ball Brothers Co Inc Rubber curing apparatus and method
US3859247A (en) * 1970-11-20 1975-01-07 Gen Electric Pressureless cure system for chemically cross-linking ethylene containing polymers
US3946099A (en) * 1972-11-10 1976-03-23 General Electric Company Pressureless cure system for chemically cross-linking ethylene containing polymers, to form an insulated conductor
US4155965A (en) * 1977-01-07 1979-05-22 The Dow Chemical Company Continuous submerged foaming of thermoplastic resin
US4209484A (en) * 1977-02-28 1980-06-24 Pont-A-Mousson S.A. Method of manufacturing products of cross-linked thermoplastic material
US4226816A (en) * 1977-07-16 1980-10-07 Aisin Chemical Company, Limited Method of manufacturing a clutch facing of the type used for automotive automatic transmissions
US4143106A (en) * 1977-08-15 1979-03-06 The Dow Chemical Company Continuous flood foaming of thermoplastic resin
US4415518A (en) * 1981-12-21 1983-11-15 Pochurek Gerald M Continuous curing of cable
US4892544A (en) * 1988-03-07 1990-01-09 Dow Corning Wright Corporation Methods for forming hollow, porous-surfaced elastomeric bodies
US5595695A (en) * 1995-05-30 1997-01-21 Sealex Inc. Process for preparing matte finish elastomer
EP0985509A1 (en) * 1998-05-04 2000-03-15 COLMEC S.p.A. Method and apparatus for the curing of extruded sections on a bath of melted salts

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